CN108993332A - A kind of preparation method of heat-resisting essence micro-capsule - Google Patents
A kind of preparation method of heat-resisting essence micro-capsule Download PDFInfo
- Publication number
- CN108993332A CN108993332A CN201810845871.1A CN201810845871A CN108993332A CN 108993332 A CN108993332 A CN 108993332A CN 201810845871 A CN201810845871 A CN 201810845871A CN 108993332 A CN108993332 A CN 108993332A
- Authority
- CN
- China
- Prior art keywords
- essence
- preparation
- capsule
- added
- heat
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
- B01J13/046—Making microcapsules or microballoons by physical processes, e.g. drying, spraying combined with gelification or coagulation
Abstract
A kind of preparation method of heat-resisting essence micro-capsule includes the following steps: that (1) will be added drop-wise in the first ethanol water after the mixing of esters of silicon acis, alkali and dehydrated alcohol and-polycondensation reaction is hydrolyzed at a certain temperature, SiO is made2Colloidal sol；(2) essence is added in solvent and is uniformly mixed, surfactant is then added, make its alkaline system with aqueous slkali adjusting；(3) step (2) is obtained into alkaline system and is added to the SiO that step (1) obtains2After mixing a period of time in colloidal sol, by the separation of obtained suspension washed with water repeatedly to neutrality, solids is obtained；(4) step (3) is obtained after solids washs separation repeatedly with the second ethanol water, obtained solids is dried in vacuo to get the heat-resisting essence micro-capsule.Essence microcapsule preparation method of the invention is simple, and essence microencapsulated flavor utilization rate obtained is high.Fragrance under the conditions of temperature is 90 DEG C or so of essence micro-capsule made from preparation method of the invention is stable, lasting is lasting.
Description
Technical field
The invention belongs to be sustained essence preparing technical field, and in particular to a kind of sol-gel system of heat-resisting essence micro-capsule
Preparation Method.
Background technique
Essence can be perceived by human body rapidly as a kind of stronger substance of volatility, but duration is generally poor.
Slow release technology is a kind of substance control release technic, by carrying out certain processing to object or relying on auxiliary material
A certain special nature make object release medium in slowly or controllably discharge.By being carried out at slow controlled release to spices and essence
Reason can achieve the purpose for extending and releasing the fragrant time, while also can reach the auxiliary such as other improvement spices and essence thermal stability
Purpose.Micro-capsule is a kind of slow control delivery of relatively common typical reservoir devices spices and essence, is made of cyst wall and inner core two parts,
Some natural or synthetic high molecular materials are generallyd use as cyst wall, such as natural gum glue, gelatin, chitosan, β-ring paste
Essence and cellulose etc..The heat resistance of this kind of microcapsule essence is poor.
Silicon materials are also more typical one of support materials.Silicon materials have good biocompatibility and stable structure
Property, due to the development of surfactants' templating in recent years, preparing for silicon-based mesoporous material is more convenient, and aperture and shape
It is adjustable, it is one of optimal slow controlled release carrier.
The present invention is for the first time prepared the wall material that silicon materials are used for essence micro-capsule.
Summary of the invention
It is an object of the invention to the deficiencies that the heat resistance for prior art essence microcapsule is poor, provide a kind of molten
Glue-gel prepares essence micro-capsule method and its application.
The present invention using ethyl orthosilicate (TEOS) as wall material presoma, essence as core material, 2-methyl cellosolve and go from
Sub- water is cosolvent system, and using alkali as catalyst, cetab and dodecyl trimethyl ammonium bromide are mixing
Template prepares heat resistance mesopore silicon oxide essence micro-capsule by sol-gel method at room temperature, judges to wrap by thermogravimetric analysis
Bury the release temperature and burst size of flavors and fragrances.Preparation method preparation process of the invention is simple, essence microcapsule heat obtained
Stability is high, essence utilization rate is high.
The purpose of the present invention is achieved by the following technical programs.
First aspect present invention discloses a kind of preparation method of heat-resisting essence micro-capsule, includes the following steps:
(1) it is added drop-wise in the first ethanol water after mixing esters of silicon acis, alkali and dehydrated alcohol and carries out at a certain temperature
SiO is made in hydrolysis-condensation reaction2Colloidal sol；
(2) essence is added in solvent and is uniformly mixed, surfactant is then added, make its alkali with aqueous slkali adjusting
Property system；
Step (1) and (2) are in no particular order；
(3) step (2) is obtained into alkaline system and is added to the SiO that step (1) obtains2After mixing a period of time in colloidal sol,
By the separation of obtained suspension washed with water repeatedly to neutrality, solids is obtained；
(4) step (3) is obtained after solids washs separation repeatedly with the second ethanol water, obtained solids vacuum
Drying is to get the heat-resisting essence micro-capsule.
Preferably, esters of silicon acis described in step (1) is ethyl orthosilicate, and first ethanol water is 50wt% ethyl alcohol
Aqueous solution；The hydrolysis-condensation reaction temperature is 60 DEG C -80 DEG C.
Preferably, essence described in step (2) is menthol, lemon extract, orange flavor, lily essence or flavoring rose essence
One or more of, the solvent is 2-methyl cellosolve aqueous solution；The surfactant is cetyltrimethylammonium
Ammonium and dodecyl trimethyl ammonium bromide mixture；It is 11~13 that the alkalinity, which is pH value,.
Preferably, the second ethanol water described in step (4) is 75wt% ethanol water；Described is vacuum drying
Temperature is 40~50 DEG C, 24~48h of time.
Second aspect of the present invention discloses the heat-resisting essence micro-capsule of the preparation method preparation for the use in tobacco product
On the way.
A kind of specific preparation method of heat-resisting essence micro-capsule of the invention, the specific steps are as follows:
(1) ethyl orthosilicate of 50mL, 0.1mol/L sodium hydroxide 30mL and dehydrated alcohol 30mL are mixed, is stirred at room temperature
It mixes, 50wt% ethanol water 30mL is then added dropwise ,-polycondensation reaction is hydrolyzed, be warming up to 70 DEG C after reacting 1h, constant temperature polymerization
SiO is made in 2h2Colloidal sol；
(2) 1~2g essence (one of menthol, lemon extract, orange flavor, lily essence or flavoring rose essence) is added
The in the mixed solvent for entering the 2-methyl cellosolve and 120~150mL deionized water to 210~250mL, stirs 10- at room temperature
30min；Then 2.5~3.0mg cetab and the dodecyl trimethyl ammonium bromide of 2.1~2.5mg is added
Mixture, being adjusted to pH value with 0.1mol/L sodium hydroxide solution is 11~13, stirs 20-40min at room temperature, obtains alkaline body
System；
Step (1) and (2) are in no particular order；
(3) step (2) is obtained into alkaline system and is added to the SiO that step (1) obtains2In colloidal sol, stir at room temperature for 24 hours,
It will obtain suspension and deionized water 10~20min of ultrasonic treatment is added, and be washed, be centrifuged repeatedly, until supernatant pH value connects
Weakly acidic pH；Centrifugal rotational speed is 3500~6000r/min, and the time is 10~20min；Obtain solids；
(4) step (3) is obtained into solids and 75wt% ethanol water is added, the additional amount of 75wt% ethyl alcohol is solids
The 50~100 of quality, stir 2~3h, and suction filtration obtains solids；Repeat this step 2-3 time, by solids vacuum drying to get
Heat-resisting essence micro-capsule；40~50 DEG C of vacuum drying, 24~48h of time.
By the heat-resisting essence micro-capsule of preparation by thermogravimetric analysis, the temperature of thermogravimetric analysis is 50 DEG C~120 DEG C, judges micro-capsule
The release temperature and burst size of middle essence.
Fragrance is stable, lasting is lasting for that can make in tobacco product for the heat-resisting essence micro-capsule of the preparation method preparation
And uniformly.
Beneficial effects of the present invention:
1, preparation method of the invention using mixed surfactant as template, 2-methyl cellosolve and water be cosolvent,
Sodium hydroxide is catalyst, and ethyl orthosilicate is precursor preparation SiO2Colloidal sol has by material prepared by sol-gel method
Porous network structure.
2, preparation method of the invention be made heat-resisting essence micro-capsule with temperature be 90 DEG C or so under the conditions of fragrance it is stable,
Fragrance lasting feature.For stablizing fragrance release, lasting is lasting and uniform, and the utilization rate of essence is obvious
It improves.
3, preparation method of the invention carries out the removal of template using extraction, remains the essence in micro-capsule.This hair
Bright essence microcapsule preparation method is simple, and essence microencapsulated flavor utilization rate obtained is high.
Detailed description of the invention
Fig. 1 is essence thermal gravimetric analysis curve.A curve is the thermogravimetric curve of menthol；B curve is the resistance to of the preparation of embodiment 1
The thermogravimetric curve of hot essence micro-capsule.
Specific embodiment
Method of the invention is further described below with reference to embodiment, but protection scope of the present invention is not limited to
This.
Embodiment 1: the heat-resisting essence micro-capsule preparation of menthol.
(1) ethyl orthosilicate of 50mL, 0.1mol/L sodium hydroxide 30mL and dehydrated alcohol 30mL are mixed, is stirred at room temperature
It mixes, 50wt% ethanol water 30mL is added dropwise ,-polycondensation reaction is hydrolyzed, be warming up to 70 DEG C after reacting 1h, constant temperature polymerize 2h, system
Obtain SiO2Colloidal sol；
(2) 1g menthol is added to the in the mixed solvent of 2-methyl cellosolve 210mL and deionized water 120mL, room temperature
Lower stirring 10min；The cetab of 2.5mg and the dodecyl trimethyl ammonium bromide mixture table of 2.1mg is added
Face activating agent, adjusting pH value with 0.1mol/L sodium hydroxide solution is 11~13, stirs 20min at room temperature and obtains alkaline system；
Step (1) and (2) are in no particular order；
(3) SiO for preparing step (1)2Colloidal sol is added in the alkaline system of step (2), is stirred for 24 hours, is obtained at room temperature
To suspension be added deionized water be ultrasonically treated 10min, then 3500r/min be centrifuged 20min, obtain solid deionized water into
Row washing is then centrifuged for separating, and washing centrifugation is multiple, until supernatant pH value obtains solids close to neutrality；
(4) the 75wt% ethanol water of 50 times of weight is added in the solids for obtaining step (3), stirs 2h, then takes out
Filter obtains solids, repeats this step 2-3 times；24~48h is dried in vacuo at 40~50 DEG C of obtained solids to get described in
Heat-resisting essence micro-capsule；
(5) the heat-resisting essence micro-capsule for obtaining step (4) carries out thermogravimetric analysis, and the temperature of thermogravimetric analysis is 50 DEG C~120
DEG C, thermal gravimetric analysis results are shown in Fig. 1.Fig. 1 is essence thermal gravimetric analysis curve, and wherein a curve is the thermogravimetric curve of menthol；B curve
For the thermogravimetric curve of heat-resisting essence micro-capsule prepared by embodiment 1.By a curve of Fig. 1 it is found that menthol decomposes acutely, 67 DEG C of left sides
Right essence starts violent weightlessness, and when to 110 DEG C, weight-loss ratio reaches 82%；By the b curve of Fig. 1 it is found that capsule is fragrant before 110 DEG C
Essence is lost slightly, caused by this is the essence adhered to as solvent remaining in sample and surface；110 DEG C -125 DEG C, capsule
The thermogravimetric weight loss highest of essence, temperature reaches the fusing point of wall material at this time, and capsule essence starts gradually to decompose as the temperature rises.
Therefore from Fig. 1 it can be found that heat-resisting essence micro-capsule made from the present embodiment is when temperature is lower than 110 DEG C, the loss of component compared with
It is few；Since 110 DEG C, essence starts to volatilize, until essence volatilization reaches balance at 150 DEG C.Heat-resisting essence micro-capsule obtained it is resistance to
Thermal effect is obviously improved.
Heat-resisting essence micro-capsule obtained is used in tobacco product, fragrance stabilization, lasting can be made persistently and uniform.
Embodiment 2: the heat-resisting essence micro-capsule preparation of lemon extract
(1) with 1 step of embodiment (1)；
(2) 2g lemon extract is added to the in the mixed solvent of 2-methyl cellosolve 250mL and deionized water 150mL, room temperature
Lower stirring 20min；The cetab of 3.0mg and the dodecyl trimethyl ammonium bromide mixture table of 2.5mg is added
Face activating agent, adjusting pH value with 0.1mol/L sodium hydroxide solution is 11~13, stirs 30min at room temperature；
Step (1) and (2) are in no particular order；
(3) SiO for preparing step (1)2Colloidal sol is added in step (2), is stirred at room temperature for 24 hours, is obtained suspension and is added
Enter deionized water ultrasonic treatment 15min, 5000r/min be centrifuged 15min, obtain solid with deionized water carry out washing be then centrifuged for
Separation, washing centrifugation is multiple, until supernatant pH value obtains solids close to neutrality；
(4) the 75wt% ethyl alcohol of 50 times of weight is added in the solids for obtaining step (3), stirs 2h, then filters and obtains
Solids repeats this step 2-3 times；24~48h is dried in vacuo at 40~50 DEG C of obtained solids to get to described heat-resisting
Essence micro-capsule；
(5) the heat-resisting essence micro-capsule for obtaining step (4) carries out thermogravimetric analysis, and the temperature of thermogravimetric analysis is 50 DEG C~120
℃.As a result for when temperature is lower than 115 DEG C, the loss of component is less；Since 115 DEG C, essence starts to volatilize, until at 160 DEG C,
Essence volatilization reaches balance.The heat-resisting effect of heat-resisting essence micro-capsule obtained is obviously improved.
Heat-resisting essence micro-capsule obtained is used in tobacco product, fragrance stabilization, lasting can be made persistently and uniform.
Embodiment 3: the heat-resisting essence micro-capsule preparation of lily essence.
(1) with 1 step of embodiment (1)；
(2) 1.5g lily essence is added to the in the mixed solvent of 2-methyl cellosolve 230mL and deionized water 130mL, room
Temperature is lower to stir 30min；The dodecyl trimethyl ammonium bromide mixing of the cetab and 2.3mg of 2.8mg is added
Surfactant, adjusting pH value with 0.1mol/L sodium hydroxide solution is 11~13, stirs 40min at room temperature；
(3) SiO for preparing step (1)2Colloidal sol is added in step (2), is stirred at room temperature for 24 hours, is obtained suspension and is added
Enter with deionized water be ultrasonically treated 20min, 6000r/min be centrifuged 10min, obtain solid with deionized water wash then from
Heart separation, washing centrifugation is multiple, until supernatant pH value obtains solids close to neutrality；
(4) the 75wt% ethyl alcohol of 50 times of weight is added in the solids for obtaining step (3), stirs 2h, then filters and obtains
Solids repeats this step 2-3 times；24~48h is dried in vacuo at 40~50 DEG C of obtained solids to get to described heat-resisting
Essence micro-capsule；
(5) the heat-resisting essence micro-capsule for obtaining step (4) carries out thermogravimetric analysis, and the temperature of thermogravimetric analysis is 50 DEG C~120
℃.As a result for when temperature is lower than 120 DEG C, the loss of component is less；Since 120 DEG C, essence starts to volatilize, until at 160 DEG C,
Essence volatilization reaches balance.The heat-resisting effect of heat-resisting essence micro-capsule obtained is obviously improved.
Heat-resisting essence micro-capsule obtained is used in tobacco product, fragrance stabilization, lasting can be made persistently and uniform.
Claims (5)
1. a kind of preparation method of heat-resisting essence micro-capsule, which comprises the steps of:
(1) it is added drop-wise in the first ethanol water after mixing esters of silicon acis, alkali and dehydrated alcohol and reacts at a certain temperature,
SiO is made2Colloidal sol；
(2) essence is added in solvent and is uniformly mixed, surfactant is then added, make its alkaline body with aqueous slkali adjusting
System；
Step (1) and (2) are in no particular order；
(3) step (2) is obtained into alkaline system and is added to the SiO that step (1) obtains2After mixing a period of time in colloidal sol, it will obtain
Suspension washed with water separation repeatedly to neutral, obtain solids；
(4) step (3) is obtained into obtained solids vacuum drying after solids washs separation repeatedly with the second ethanol water
Up to the heat-resisting essence micro-capsule.
2. preparation method according to claim 1, which is characterized in that esters of silicon acis described in step (1) is ethyl orthosilicate,
First ethanol water is 50wt% ethanol water；The temperature of the reaction is 60 DEG C -80 DEG C.
3. preparation method according to claim 1, which is characterized in that essence described in step (2) is menthol, lemonene
One or more of essence, orange flavor, lily essence or flavoring rose essence, the solvent are 2-methyl cellosolve aqueous solution；Institute
Stating surfactant is cetab and dodecyl trimethyl ammonium bromide mixture；The alkalinity for pH value is
11~13.
4. preparation method according to claim 1, which is characterized in that the second ethanol water described in step (4) is
75wt% ethanol water；The vacuum drying temperature is 40~50 DEG C, and the time is 24~48h.
5. the heat-resisting essence micro-capsule of preparation method preparation according to claim 1 to 4 is for the use in tobacco product
On the way.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810845871.1A CN108993332B (en) | 2018-07-27 | 2018-07-27 | Preparation method of heat-resistant essence microcapsule |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810845871.1A CN108993332B (en) | 2018-07-27 | 2018-07-27 | Preparation method of heat-resistant essence microcapsule |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108993332A true CN108993332A (en) | 2018-12-14 |
| CN108993332B CN108993332B (en) | 2021-07-13 |
Family
ID=64598080
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810845871.1A Active CN108993332B (en) | 2018-07-27 | 2018-07-27 | Preparation method of heat-resistant essence microcapsule |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108993332B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103263877A (en) * | 2013-05-17 | 2013-08-28 | 义乌市中力工贸有限公司 | Preparation method of essential oil-contained silicon dioxide microcapsule |
| CN103328621B (en) * | 2011-07-04 | 2014-07-02 | 丽华（广州）香精有限公司 | Nano-flavor and preparation method thereof |
| CN104031740A (en) * | 2014-05-30 | 2014-09-10 | 上海应用技术学院 | Heat-resistant rose essence capsule and preparation method thereof |
| CN104449590A (en) * | 2014-12-05 | 2015-03-25 | 中国工程物理研究院化工材料研究所 | Phase-change energy-storage material nanocapsule and preparation method thereof |
-
2018
- 2018-07-27 CN CN201810845871.1A patent/CN108993332B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103328621B (en) * | 2011-07-04 | 2014-07-02 | 丽华（广州）香精有限公司 | Nano-flavor and preparation method thereof |
| CN103263877A (en) * | 2013-05-17 | 2013-08-28 | 义乌市中力工贸有限公司 | Preparation method of essential oil-contained silicon dioxide microcapsule |
| CN104031740A (en) * | 2014-05-30 | 2014-09-10 | 上海应用技术学院 | Heat-resistant rose essence capsule and preparation method thereof |
| CN104449590A (en) * | 2014-12-05 | 2015-03-25 | 中国工程物理研究院化工材料研究所 | Phase-change energy-storage material nanocapsule and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 邓春晖等著: "《磁性微纳米材料在蛋白质组学中的应用》", 31 December 2017, 复旦大学出版社 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108993332B (en) | 2021-07-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101456569B (en) | Method for quickly preparing aerogel by hydro-thermal synthesis at low cost | |
| WO2018049965A1 (en) | Method for quickly preparing aerogel by using microemulsion as precursor | |
| CN107447297B (en) | A kind of hydrogel alginate fibre and preparation method thereof | |
| CN107522389B (en) | Micro-nano bioactive glass microsphere with surface nano-pore structure and preparation method thereof | |
| CN108940148A (en) | A kind of preparation method of temperature control sustained-release essence micro-capsule | |
| CN109504537A (en) | Mesoporous silicon dioxide nano fragrance of temperature control sustained-release and preparation method thereof | |
| CN108017062A (en) | Hydrophobic silica aerogel and preparation method thereof | |
| CN104073346A (en) | Nanometer level microcapsule sweet orange essence and preparing method thereof | |
| JP2019529326A (en) | Method for producing silica airgel blanket, and silica airgel blanket produced thereby | |
| CN108531292A (en) | Preparing spherical SiO 2 nanometer fragrance of light-operated sustained release and preparation method thereof | |
| CN109574021A (en) | A method of Metaporous silicon dioxide material is prepared by template of hydroxyethyl cellulose | |
| RU2002131904A (en) | INHIBITED WATER-SOLUBLE SIMPLE ETHER OF CELLULOSE AND METHOD OF ITS PRODUCTION | |
| CN105926287A (en) | Purely-natural and mosquito-repelling fabric for infants and production method of purely-natural and mosquito-repelling fabric | |
| CN109422919A (en) | A kind of preparation method of aluminium oxide-chitosan aerogel composite | |
| CN106905437A (en) | Heat-resisting redispersible powder Cellulose nanocrystal high and preparation method thereof | |
| CN108993332A (en) | A kind of preparation method of heat-resisting essence micro-capsule | |
| CN106592253A (en) | Fragrant wool fiber and preparation method thereof | |
| CN107308499A (en) | Nanometer biological glass/polymer three-dimensional porous material and its preparation method and application | |
| CN110156038A (en) | A kind of micropore-mesopore-macropore multi-stage porous SBA-15 molecular sieve and its preparation method and application | |
| CN109908396A (en) | A kind of calcium ion-exchanged porous-starch hemostatic material and its preparation method and application | |
| CN108175718A (en) | A kind of sun-proof camellia of heat-resistance antibacterial with long-term sustained release effect receives microcapsules and preparation method thereof | |
| CN110339814A (en) | Modified dioxide composite silica aerogel of methyl with hierarchical porous structure and its preparation method and application | |
| CN103803560B (en) | A kind of bending bar-shaped mesoporous SiO 2and preparation method thereof | |
| CN109294563A (en) | A kind of super-small fluorescence mesoporous organic silicon oxide probe and preparation method and application | |
| CN109303879A (en) | A kind of traditional Chinese medicine plaster and preparation method thereof for treating eczema |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |